HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Sulfuric Acid → 1,2,4-Triazolo(4,3-a)pyridin-3(2H)-one
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Sulfuric Acid | HCID 1118 | — |
| Edukt | 2-Chloropyridine | HCID 7977 | — |
| Edukt | Glycol monoethyl ether | HCID 8076 | — |
| Edukt | Semicarbazide hydrochloride | HCID 11236 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Produkt | 1,2,4-Triazolo(4,3-a)pyridin-3(2H)-one | HCID 81431 | 59% |
Reaktionsschritte
A mixture of 50 g. (0.44 mole) of 2-chloropyridine and 98.22 g. (0.88 mole) of semicarbazide hydrochloride in 150 ml. of 2-ethoxyethanol was heated to reflux and then treated with a solution of 1 ml. of concentrated sulfuric acid (36 N) in 5 ml. of 2-ethoxyethanol. The resulting solution was refluxed for 18 hr., cooled to about 60°, and treated with 150 ml. of water. The mixture was stirred, cooled to 0°, and kept 0.5 hr. and the solid was collected on a filter. The solid was washed well with water and dried under reduced pressure, to give 35.0 g (59%) of product, m.p. 230°-231°, which was sufficiently pure to be used for the next step.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US04254124 |
| Quelldatensatz | uspto-grants-1981_03 |
| ORD ID | ord-3d13aa21801e4a6d9fde56452d9bf418 |
| Quellennotiz | uspto-grants-1981_03 |